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Acetic Acid → HCID 135705340、化合物

HRID 442219
ノート
印刷プレビュー

反応式

HRID 442219 の反応式
[NH2:1][C:2]1[C:11]([C:12]([NH2:14])=[O:13])=[C:10]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[C:21](OCC)(=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23].C(O)(=O)C>CCOCC>[C:15]1([C:10]2[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=[C:2]3[N:1]=[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[NH:14][C:12](=[O:13])[C:11]=23)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 176Acetic AcidHCID 7268Diethyl OxalateHCID 218217142-Amino-4-phenyl-3-quinolinecarboxamide

生成物 1

HCID 135705340HCID 135705340、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 2-amino-4-phenylquinoline-3-carboxamide (263 mg., 1.0 millimole), diethyl oxalate (5 ml.) acetic acid (5 ml.) is heated to reflux overnight. It is then cooled, diluted with ether (50 ml.) and the brown solid which forms filtered off. The filtrate is evaporated in vacuo and the oily residue triturated with saturated aqueous sodium bicarbonate solution. The resulting solid (110 mg.) is recovered by filtration and recrystallized from hot ethyl acetate (8 ml.). A small amount of insoluble material is filtered off from the hot solution. Upon cooling, the title product separates as crystals (25 mg.). M.P. = 255° C. (dec.).

後処理

  1. temperatureis heated
  2. temperatureto reflux overnight
  3. temperatureIt is then cooled
  4. filtrationthe brown solid which forms filtered off
  5. customThe filtrate is evaporated in vacuo
  6. customthe oily residue triturated with saturated aqueous sodium bicarbonate solution
  7. filtrationThe resulting solid (110 mg.) is recovered by filtration
  8. customrecrystallized from hot ethyl acetate (8 ml.)
  9. filtrationA small amount of insoluble material is filtered off from the hot solution
  10. temperatureUpon cooling

出典と根拠

ORDレコード
ord-13a5b2abc6f84712b6ae56bfbe3fface
出典データセット
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04044134

反応ノート

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